++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:16:45 on 09-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.373 19.144 20.249 90.00 78.59 90.00 9938 Reflections read from file s92.hkl; mean (I/sigma) = 9.40 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5000 4892 4954 4978 7423 6639 6627 9938 N (int>3sigma) = 0 3516 3368 3578 3634 5231 4753 4758 7160 Mean intensity = 0.0 61.3 43.7 61.9 62.2 55.7 63.3 61.9 61.1 Mean int/sigma = 0.0 9.3 8.7 9.4 9.5 9.1 9.5 9.4 9.5 Lattice type: P chosen Volume: 3561.48 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 9.373 19.144 20.249 90.00 78.59 90.00 Niggli form: a.a = 87.85 b.b = 366.49 c.c = 410.03 b.c = 0.00 a.c = 37.56 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.054 [ 7515] Cell: 9.373 19.144 20.249 90.00 101.41 90.00 Volume: 3561.48 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5000 4892 4954 4978 7423 6627 6639 9938 N (int>3sigma) = 0 3516 3368 3578 3634 5231 4758 4753 7160 Mean intensity = 0.0 61.3 43.7 61.9 62.2 55.7 61.9 63.3 61.1 Mean int/sigma = 0.0 9.3 8.7 9.4 9.5 9.1 9.4 9.5 9.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.998 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 21 269 261 272 N I>3s 4 99 14 101 3.5 13.5 1.6 13.4 1.9 4.5 1.0 4.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.054 7515 1.9 / 4.4 3.48 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C15H20F3N2O3Pd Formula weight = 439.73 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.640, non-H atomic volume = 18.5 and following cell contents and analysis: C 120.00 40.97 % H 160.00 4.58 % N 16.00 6.37 % O 24.00 10.92 % F 24.00 12.96 % Pd 8.00 24.20 % F(000) = 1768.0 Mo-K(alpha) radiation Mu (mm-1) = 1.09 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in P2(1)/c CELL 0.71073 9.3727 19.1440 20.2492 90.000 101.414 90.000 ZERR 8.00 0.0009 0.0015 0.0019 0.000 0.000 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O F PD UNIT 120 160 16 24 24 8 TREF HKLF 4 END -------------------------------------------------------------------------------